Determination Of Ruthenium Research Articles

Determination of ruthenium in borosilicate glasses by inductively coupled plasma mass spectrometry

Determination of ruthenium in borosilicate glasses by inductively coupled plasma mass spectrometry

Determination of Ruthenium in Ion exchange membranes by Energy Dispersive X-ray Fluorescence (EDXRF)

Determination of Ruthenium in Ion exchange membranes by Energy Dispersive X-ray Fluorescence (EDXRF)

Solvent extraction separation and spectrophotometric determination of ruthenium(III) with p-methylphenyl thiourea: sequential separation of ruthenium, osmium and iron

ABSTRACT A selective and sensitive solvent extraction and spectrophotometric study of the ruthenium(III)–p-methylphenyl thiourea (PMPT) system is presented. The optimum conditions were determined by a critical study of acid concentration, reagent concentration, equilibration period, heating time and effect of solvent on the equilibrium. Ruthenium(III) forms 1:1 complex with PMPT in 20% ethanol and extracted into chloroform. Conformity to Beer’s law at 600 nm was observed up to 40 µg mL–1 of ruthenium. Molar absorptivity and Sandell’s sensitivity were found to be 2.31 × 103 L mol−1cm−1 and 0.044 μg cm−2, respectively. The detection limits were 0.11 μg mL−1 of ruthenium. The method is free from interferences from large number of cations and anions. Proposed method was successfully applied to the separation and determination of ruthenium from synthetic alloys, catalyst and water samples. Sequential separation and determination method for ruthenium(III), osmium(VIII) and iron(II) has been developed.

ANALYSIS OF CORROSION-RESISTANT TITANIUM ALLOYS DOPED WITH RUTHENIUM BY ICP-AES

We present a technique of multi-element analysis of new corrosion-resistant titanium alloys doped with ruthenium using Optima 7300 DV ICP-AES spectrometer (Perkin Elmer Corporation, USA) and microwave system Speedwave FOUR (Berghof Products, Germany). Compositions of the acid mixture as well as the temperature and time parameters of the sample preparation of titanium alloys under microwave heating in an autoclave which ensure a complete quantitative transfer of the sample into a convenient analytical form for subsequent ICP-AES analysis without loss of volatile components are substantiated. Optimal conditions of excitation of the analytical signal of analytes for ICP-spectrometer are specified and analytical lines of the elements free of spectral interference are chosen for determination of all critical components in corrosion-resistant titanium alloys. The studies were carried out using samples of experimental melting of industrial titanium alloys of different classes, which, due to volumetric doping with ruthenium, are under development and are not yet commercially available in Russia (grades of alloys PT-7M+Ru, PT-3B+Ru, 5B+Ru, 37+Ru, BT-22+Ru). The samples contained the following alloying elements (% wt.): Al (1.8 – 6.3); V (1.0 – 5.5); Mo (0.7 – 5.5); Zr (0.2 – 3.0); Cr (0.5 – 1.5); Fe (0.5 – 1.5); Ru (0.05 – 0.15). The correctness of the alloying element determination is confirmed by analysis of standard samples using the method of sample variation and spike test for ruthenium determination. The developed technique significantly shortens the duration of the analysis due to combination of the multi-element method of ICP-AES with microwave sample preparation, expands the list of detectable elements in titanium alloys, and increases the accuracy of Al, Si, V, Cr, Fe, Ni, Cu, Zr, Nb, Mo and Ru determination in titanium alloys in critical(rated) ranges of concentrations.

Improved method for spectrophotometric determination of ruthenium using 1,10-phenanthroline: application for analysis of complex compounds

A day-to-day fast, cheap and accurate analysis of ruthenium in complex compounds without forgoing distillation of ruthenium tetroxide was conducted.

Extractive Spectrophotometric Determination of Ruthenium (III) Using Novel Salen Ligand

Extractive Spectrophotometric Determination of Ruthenium (III) Using Novel Salen Ligand

Rhenium and ruthenium determination in nanostructured high-temperature alloys for aerospace engineering

Various methods for sampling preparation in the analysis of high-temperature nickel-based alloys (acid dissolving and alloying) are described. It is shown that the optimum method for transfer of rheniumand ruthenium-containing samples into solution is dissolving in sulfuric acid with addition of hydrogen peroxide and utilization of a 20% NaOH solution as an absorbent. The technique requires no separation or masking of components of the sample base. The validity of test results was checked by methods for variation in the charge and additives and by comparison with data of other analysis methods.

SPECTROPHOTOMETRIC DETERMINATION OF RUTHENIUM PRESENT IN TRACES

Phenanthraquinone monothiosemicarbazone (PTS) has been used in the determination of ruthenium by spectrophotometric method. PTS forms a green complex with ruthenium (III ) at pH 5.2 to 6.7. The complex is soluble in DMF. The maximum absorbance of the complex has been found at 660 nm. The complex has been found to obey Beers Law up to 9.38 ppm. Effect of diverse ions in the determination of ruthenium has also been studied. Attempts have been made to mask the various interfering cations by anions. The sensitivity of the method is 0.0102 μg Ru/cm 2 at 660 nm Keywords— DMF, Phenanthraquinone monothiosemicarbazone (PTS), ruthenium (III), spectrophotometric --------------------------------------------------------------------***------------------------------------------------------------------

Determination of Ruthenium in Waste Ruthenium Catalysts Using Inductively Coupled Plasma Optical Emission Spectrometry after Sample Digestion by High Temperature Fusion

A technique for determination of Ru in waste ruthenium catalysts using ICP-OES after sample digestion by high temperature fusion with NaOH-NaNO3mixture was described. Such experiment conditions were investigated as the influence of sample digestion methods, fusion time, fusion temperature, the dosage of NaOH-NaNO3mixture and interfering ions on the determination. Under the optimized conditions, the limits of detection (LODs) of Ru for tested solutions were 10 ng mL-1. The relative standard deviations (RSDs) for Ru were 2.01 (CRu= 1 mg L-1, n = 7). The linear ranges of calibration graphs for Ru were 0 ~ 100.00 mg L-1. The proposed method was applied to determine the practical samples with good recoveries and satisfactory results.

Simultaneous Determination of Ruthenium and Zinc in Catalysts for Hydrogenation of Benzene to Cyclohexene Using Sodium Peroxide Fusion Sample Digestion and ICP-OES

A novel method for simultaneous determination of ruthenium and zinc in catalysts for hydrogenation of benzene to cyclohexene was established by inductively coupled plasma optical emission spectrometry after sample digestion by high temperature fusion with Na2O2. Such experiment conditions were investigated as the influence of sample digestion methods, fusion time, fusion temperature, the dosage of Na2O2 and interfering ions on the determination. Under the optimized conditions, the limits of detection (LODs) of Ru and Zn for tested solutions were 11 and 13 ng mL-1, respectively. The relative standard deviations (RSDs) for Ru and Zn were 2.01 and 2.35 % (CRu, Zn = 1 mg L-1, n = 7), respectively. The linear ranges of calibration graphs for Ru and Zn were 0.05 ~ 100.00 mg L-1 and 0.04 ~ 50.00 mg L-1, respectively. The proposed method was applied to determine catalyst samples with good recoveries and satisfactory results.

Determination of Ruthenium in Waste Ruthenium-Loaded Carbon Catalyst Samples Using Teflon Pressure Vessel-Assisted Sample Digestion and ICP-OES

A novel method for the determination of ruthenium in waste ruthenium-loaded carbon catalyst samples was established by inductively coupled plasma optical emission spectrometry after samples digested by Teflon pressure digestion vessel with aqua regia. Such experiment conditions were investigated as the influence of sample dissolution methods, digestion time, digestion temperature and interfering ions on the determination. Under the optimized conditions, the limit of detection (LODs) of Ru for tested solution was 9 ng mL-1. The relative standard deviations (RSDs) for Ru was 2.12 % (CRu= 1 mg L-1, n = 7). The linear range of calibration graph for Ru and Zn was 0 ~ 100.00 mg L-1. The proposed method was applied to determine the practical samples with good recoveries and satisfactory results.

Simultaneous Determination of Ruthenium, Zinc and Zirconium in Waste Zirconium Dioxide Loaded Ruthenium-Zinc Catalysts Using Inductively Coupled Plasma Optical Emission Spectrometry

A technique for simultaneous determination of Ru, Zn and Zr in waste Ru-Zn/ZrO2catalysts using ICP-OES after sample digestion by high temperature fusion with KOH-KNO3mixture was described. Such experiment conditions were investigated as the influence of sample digestion methods, fusion time, fusion temperature, the dosage of KOH-KNO3mixture and interfering ions on the determination. Under the optimized conditions, the limits of detection (LODs) of Ru, Zn and Zr for tested solutions were 11, 8 and 5 ng mL-1, respectively. The relative standard deviations (RSDs) for Ru, Zn and Zr were 2.01, 2.55 and 1.92 % (CRu, Zn,Zr= 1 mg L-1, n = 7), respectively. The linear ranges of calibration graphs for Ru, Zn and Zr were 0 ~ 100.00 mg L-1, 0 ~ 50.00 mg L-1and 0~60.00 mg L-1, respectively. The proposed method was applied to determine the practical samples with good recoveries and satisfactory results.

Spectrophotometric Determination of Trace Ruthenium by its Catalytic Effect on Oxidation of Switzerland Pigment with KIO<sub>4</sub>

A spectrophotometric method for the determination of ruthenium (III) is described, based on its catalytic effect on the oxidation reaction of switerland pigment with potassium periodate in 0.016 mol/L of hydrogen chloride medium and in the presence of OP emulsifier (p-iso-octyl phenoxy polyethoxy ethanol) at 100 °C. The above reaction is followed spectrophotometrically by measuring the decrease in the absorbance at 608 nm for the catalytic reaction of switerland pigment. The calibration curve for the recommended method was linear in the concentration range over 0.041.0 μg/L and the detection limit of the method for Ru (III) is 0.012 μg/L. The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 100.48 kJ/mol. The relative standard deviation for the determination of ruthenium (III) at the concentration of 0.02 μg/25 mL is calculated to be 2.3 % (n=11). In combination with distilled separation, the method has been successfully applied for the determination of trace ruthenium (III) in some ores and metallurgy proucts with the relative standard deviations (RSD) over 2.9 %3.8 % and the recovery over 98.2 %-103.6 %.

Determination of Ruthenium in Heat-Resistant Nickel Alloys by Atomic Emission Spectrometry with Inductively Coupled Plasma

UDC 543.423 A technique for measuring 0.5-6.5 mass% ruthenium in heat-resistant nickel alloys using atomic emission spectrometry with inductively coupled plasma was developed. The measurement precision (repeatability and reproducibility) was determined. Introduction. One of the most important applications of heat-resistant nickel (Ni) alloys (HNA) is the preparation from them of aviation gas-turbine engine blades and disks. The gas temperature at the turbine intake has risen during the last 50 years of aviation development from 1200 K in second-generation engines to 1800-1950 K in fi fth-generation engines (1-3). HNA are complicated doped compounds with a heterophase structure, the principal components of which are disperse (<0.5 μm) particles of the γ'-phase based on the ordered intermetallic compound Ni3Al and a complicated doped nickel γ-solid solution. Furthermore, topologically densely packed (TDP) phases that reduce the stability of the alloy phases can form in HNA under certain crystallization and heat-treatment conditions (4). As a result, the operational properties of the alloys degrade. Rhenium (Re) (up to 5-6 mass%) was previously added to the alloy in order to stabilize the phase composition and to reduce the probability of segregating TDP phases. Doping of fi fth-generation HNA with ruthenium (Ru) was also proposed recently (5-11). This made the alloys even more heat-resistant and produced several defi nite advantages over Re. It had almost half the density, was less prone to TDP phase formation, and practically did not sweat during crystallization. Simple, rapid, and robust analytical methods that enable Ru to be determined in alloys from 0.5 to 6.5 mass% are needed in order to monitor the Ru content in HNA during their fabrication and production. Several techniques and standards for methods of determining Ru in Pt-Ru alloys are known (12-14). However, robust, modern, and attested techniques for determining Ru in HNA at a content of 0.5-6.5% are not available in Russia. The goal of the present work was to develop a technique for measuring the Ru mass fraction (0.5-6.5 mass%) in HNA using atomic emission spectrometry with inductively coupled plasma (ICP-AES). The technical and experimental principles for using the ICP-AES method are well known (15-17). Experimental. A Varian 730-ES ICP-AES spectrometer equipped with a horizontally positioned high-temperature (up to 10,000°C) induction burner (longitudinal view) operated by a high-frequency (40 mHz) plasma system; a purged echelle polychromator (spectral range 176-785 nm) with full computer control of the plasma view point; plasma gas fl ows; and web-integrated ICP-Expert TM II software was used for the measurements. Samples of the last generations of nickel alloys with Ru content in them according to TU (technical specifi cations) and HNA ZhS 1 (containing all components except Ru) for preparing a control solution were selected for developing the measurement technique and establishing the metrological characteristics of the measured HNA Ru mass-fraction. Measurements were made using Ru emission line λ = 343.674 nm, which was free of interferences from other elements. A series of aqueous calibration solutions based on a standard sample (SS) of Ru solution (High-Purity Standards, USA) with Ru concentration 1000 mg/dm 3 were prepared in order to study the emission signal intensity as a function of solution Ru

Kinetic Spectrophotometric Determination of Ruthenium by its Catalytic Effect on the Reduction of Spadns with Sodium Hypophosphite in Micellar Media

A simple kinetic spectrophotometric method was developed for the determination of trace amounts of Ru (III). The method is based on the reduction of spadns by sodium hypophosphite (NaH2PO2) in micellar media. The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of spadns at 515 nm with a fixed-time method. The decrease in the absorbance of spadns is proportional to the concentration of Ru (III) in the range 0.40–10.0 μg/L with a fixed time of 2.5–7.0 min from the initiation of the reaction. The limit of detection is 0.12 μg/L Ru (III). The relative standard deviation for the determination of 0.10 and 0.20 μg/25mL Ru (III) was 2.3 % and 2.0 %, respectively. The method was applied to the determination of Ru (III) in some ores and metallurgy products.

Direct spectrophotometric determination of ruthenium in aqueous streams of nuclear reprocessing

A fiber optic aided spectrophotometric technique has been developed for determination of ruthenium in nitric acid medium. The developed method is simple, accurate and applicable to aqueous streams of nuclear reprocessing. The system obeys Lambert–Beer’s law at 468 nm in the concentration range of 30–360 μg/mL of ruthenium. The molar absorption coefficient, detection limit and Sandell’s sensitivity are 68.477 L Mol−1 cm−1, 31 μg/mL and 0.0124 μg/cm2 respectively. Relative standard deviation was less than 2 % and correlation coefficient was 0.9998. The results obtained by the developed procedure are in good agreement with those obtained by the standard ICP-OES method. Fission products like zirconium and strontium are not interfering. Uranium is interfering and needs prior separation by solvent extraction method. The developed method is adaptable for remote operation and on-line monitoring.

Spctrophotometric Determination of Trace Ruthenium by its Catalytic Effect on Oxidation of 3,5-DiBr-PADAP with KIO&lt;sub&gt;4&lt;/sub&gt;

A spectrophotometric method for the determination of ruthenium (III) is described, based on its catalytic effect on the oxidation reaction of 2-[(3,5-dibromo-2-pyridy)azo]-5-diethylaminophenol (3,5-diBr-PADAP) with potassium periodate in 0.008 mol/L sodium hydroxide medium and in the presence of OP emulsifier (p-iso-octyl phenoxy polyethoxy ethanol) at 100 °C. The above reaction is followed spectrophotometrically by measuring the decrease in the absorbance at 530 nm for the catalytic reaction of 3,5-diBr-PADAP. The calibration curve for the recommended method was linear in the concentration range over 0.04 µg/L–1.0 µg/L and the detection limit of the method for Ru (III) is 0.012 µg/L. The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 100.48 kJ/mol. The relative standard deviation for the determination of ruthenium (III) at the concentration of 0.02 µg/25mL is calculated to be 2.30 % (n=11). In combination with distilled separation, the method has been successfully applied for the determination of trace ruthenium (III) in some ores and metallurgy products with the relative standard deviations (RSD) over 1.8 %–2.9 % and the recovery over 98.1 %–103.1 %.

Determination of ruthenium(III) in the presence of micellar medium by derivative spectrophotometric technique

Determination of ruthenium(III) in the presence of micellar medium by derivative spectrophotometric technique

Recent Trends in Kinetics in Analytical Chemistry and Kinetic Method for Determination of Ruthenium (III) Using Aniline Blue-Acidic Chlorite Reaction

Recent trends in the kinetic rate methods in the past three decades have been concisely reviewed to show the magnanimity of the work and scope of applications in analytical chemistry. Furthermore, based on the highly selective catalytic efficiency of Ru(III) on the oxidation of aniline blue (AB+) by acidic chlorite, a fixed-time analytical procedure is described for determination of ultratrace amounts of Ru(III). The attainable lower detection limit is 2.5 ng/ml. The proposed method allows Ru(III) determination with no interference from a wide range of cations, changes in pH, and ionic strength, which is tested with a number of synthetic mixtures.

Extractive Separation and Spectrophotometric Determination of Traces of Ruthenium from Mixtures Containing Excess Platinum Group Metals

A highly selective, sensitive, and rapid method has been developed for the spectrophotometric determination of ruthenium with 5-chloro-2-hydroxythiobenzhydrazide after extraction into molten naphthalene. Ruthenium was determined in the range 1.2–4.5 ppm. The complex was stable for more than 12 h with molar absorptivity of 1.516 × 104 L mol−1 cm−1 and detection limit of 0.0066 ppm. The method was found to be selective for ruthenium in the presence of a large number of diverse ions. Ruthenium was determined in various synthetic mixtures. The method permits the sequential separation and determination of ruthenium, osmium, and platinum from their mixtures.